• 제목/요약/키워드: $^1$H-NMR spectra

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β-CD 또는 아다만탄이 결합된 루테늄(II)-터피리딘 착화합물의 제조와 초분자 조립 (Synthesis and Supramolecular Assembly of Ru(II)-Terpyridine Complexes linked with β-Cyclodextrin or Adamantyl Group)

  • 박대림;정용채;최경호;김형진
    • 대한화학회지
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    • 제51권6호
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    • pp.526-535
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    • 2007
  • 아다만탄 또는 β-cyclodextrin이 결합된 루테늄(II)-터피리딘 착화합물(8, 9, 11)을 합성하고 1H NMR, 13C NMR 및 질량분석스펙트럼으로 구조를 확인하였다. 아다만탄이 결합된 루테늄(II)-터피리딘 착화합물(8, 11) 은 물에 전혀 녹지 않으나, β-cyclodextrin 수용액에 혼합할 경우 β-cyclodextrin과의 초분자를 형성하여 물에 잘 녹아들어갔다. 비슷한 방법으로 수용액 중에서 루테늄(II)-터피리딘 착화합물(8, 11)을 각각 착화합물 9와 혼합 하였을 때, 착화합물(8, 11)의 아다만탄 부분이 루테늄 착화합물 9의 β-cyclodextrin 내부에 포접 됨으로써 안정 한 초분자를 형성하였다.

단삼(丹蔘)으로부터 항균물질의 분리 (Isolation of Antimicrobial Compounds from Salvia miltiorrhiza Bunge)

  • 한완수
    • 한국약용작물학회지
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    • 제12권3호
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    • pp.179-182
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    • 2004
  • 단삼(丹蔘)을 bioassay-directed fractionation에 의한 에탄올 추출물의 클로로포롬 분획물을 silica gel column chromatography, recycling preparative-HPLC 등을 실시하여 항균활성을 나타내는 2개의 화합물을 분리하여 이화학적 성상 및 spectra data (IR,$^1H-NMR,\;^{13}C-NMR$ 및 Mass)에 의해 각각 Cryptotanshinone과 dihydrotanshinone I으로 동정하였으며, 이들 화합물의 항균성 (MIC)은 각각 S. epidermidis에 대하며 $6.3,\;3.1\;{\mu}g/ml$와 S. pyogenes에 대해 $6.3\;{\mu}g/ml$로 비교적 높은 활성을 나타내어 항생제로서 개발 가능성을 보여주었다.

Complete Assignment of the $^H1$ and $^{13}C$ NMR Spectra of a Sucrose Ester from Euphorbia Lathyris L.

  • Jung, Min-Hwan;Kim, Hyun-Sik;Sangdoo Ahn;Kim, Cheong-Taek;Jin, Mu-Hyun;Yim, Yong-Hyeon;Kim, Young-Kook;Jong hoa Ok
    • 한국자기공명학회논문지
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    • 제4권2호
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    • pp.125-132
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    • 2000
  • The detailed $^1$H and $^{13}$ C NMR assignments of a novel sucrose isovaleryl ester isolated from the seed of Euphorbia Lathyris L., were achieved by one-and two-dimensional techniques. The new sucrose ester was characterized as an $\alpha$-D-glucopyranoside, 3,4,6-tris-O-(3-methyl-1-oxobutyl)-$\beta$-D-fructofuranosyl, 2,6-bis(3-methylbutanoate); sucrose 4,7,8,11,12-pentaisovalerate by MS and NMR experiments.

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Isolation of Handelin from Chrysanthemum boreale

  • Kang, Sam-Sik;Kim, Ju-Sun;Son, Kun-Ho;Lee, Chong-Ock;Kim, Young-Hee
    • Archives of Pharmacal Research
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    • 제19권5호
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    • pp.406-410
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    • 1996
  • The flowers of Chrysanthemum boreale afforded handelin, a unique guaianolide dimer and a mixture of n-hydrocarbons and n-hydrocarbon alcohols in addition to b-sitosterol and b-sitosterol glucoside. Detailed analysis of the $^{1}H$- and $^{13}C$-NMR spectra of handelin was carried out by the application of two-dimensional $^{1}H-^{1}H$-COSY and $^{1}H$- $^{13}C$ multiple-bond, multiple-quantum spectroscopic correlation techniques. Handelin was inactive in the in vitro anti-tumor activity.

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¹H NMR Study of the Inclusion Complexes of Chiral Aromatic Guests with β-Cyclodextrin and Its Derivatives: Discrimination of Aromatic Protons and Chiral Recognition

  • 고광희;박종목
    • Bulletin of the Korean Chemical Society
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    • 제17권11호
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    • pp.1052-1056
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    • 1996
  • The effects of β-CD, Me-β-CD, and biphenyl capped β-CD on 1H NMR spectra of mandelic acid 1, α-methylbenzylamine 2 and 2-phenylpropionic acid 3 were investigated. Enantiomeric recognition was observed for mandelic acid 1 by all the hosts used, for α-methylbenzylamine 2 by β-CD and Me-β-CD, and for 2-phenylpropionic acid 3 by Me-β-CD. In the presence of biphenyl-capped β-CD, ο-, m-, and p-protons of the phenyl groups of the guests are discriminated due to ring current of the capped biphenyl group. The splitting pattern of the phenyl protons indicates that the phenyl group of the guests is inserted into the β-CD cavity from the secondary hydroxyl side and positioned in close proximity to the capped biphenyl ring. The magnitude of the upfield shifts of H3 and H5 protons of β-CD upon binding of guests 1-3 is similar to that caused by ephedrine or pseudoephedrine, suggesting that the substitution at benzylic carbon atom has little effect on the depth of the insertion of the phenyl group into the β-CD cavity and stability of the inclusion complexes.

녹색발광 6-알킬-3-크로몬알데히드(2,2-디알킬)하이드라존 유도체의 합성 (Synthesis of 6-Alkyl-3-Chromonealdehyde(2,2-dialkyl)hydrazone Derivatives for Green Light Emitting Materials)

  • 정평진;장홍준
    • 공업화학
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    • 제21권4호
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    • pp.424-429
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    • 2010
  • 본 연구는 유기발광디바이스용(OLED) 녹색발광재료인 6-알킬-3-크로몬알데히드(2,2-디알킬)하이드라존 유도체의 합성에 관한 것으로서, 유도체들은 탈수축합반응으로 합성되었다. 이들은 전자흡인성의 6-알킬-3-크로몬알데히드류와 전자공여성의 2,2-디알킬하이드라존류의 공액구조를 가지고 있다. 합성된 물질들은 각각 FT-IR, $^1H$-NMR 스펙트럼으로부터 그의 구조적 특성을 확인하였고, 융점, 수득률에 의하여 열적 안정성, 반응성을 확인하였으며, 여기스펙트럼과 발광스펙트럼으로부터 자외가시광과 발광특성을 확인하였다.

Separation and Characterization of Water Soluble Blue Pigments Formed from Geniposide of Gardenia Fruits

  • Park, Jee-Eun;Hahn, Tae-Ryong;Paik, Young-Sook
    • Journal of Applied Biological Chemistry
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    • 제44권4호
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    • pp.190-193
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    • 2001
  • Genipin, aglycone of geniposide isolated from fruits of Gardenia jasminoides, was transformed into blue pigments through reaction with glycine and methylamine. The blue pigments formed from glycine-reacted genipin were passed through Bio-Gel P-2 resin yielding fractions GG1 and GG2, and those from methylamine-reacted genipin were separated into fractions GM1-GM4. The first eluted higher molecular-weight fractions, GG1 and GM1, had higher tinctorial strength than the later eluted lower molecular-weight fractions, GG2 and GM2-GM4, respectively. $^1H-NMR$ spectra of GG1 and GM1 showed very broad peaks indicating that structures of the pigments were highly polymeric. $^1H-NMR$ spectra of GG2, GM3, and GM4 showed several sharp peaks at aliphatic and aromatic regions with accompanying broad peaks, although the spectrum of GM2 was rather simple. Determination of the structural and physical nature of the isolated pigments is in progress.

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녹색발광 3-크로몬알데히드(2,2-이치환)하이드라존 유도체의 합성 (Synthesis of 3-Chromonealdehyde(2,2-disubstituted)hydrazone Derivatives for Green Light Emitting Materials)

  • 정평진;장흥준
    • 공업화학
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    • 제20권6호
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    • pp.670-674
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    • 2009
  • 본 연구는 유기발광디바이스용(OLED) 녹색형광물질인 3-크로몬알데히드(2,2-이치환)하이드라존 유도체의 합성에 관한 것으로서, 유도체들은 탈수축합반응으로 합성되었다. 이들은 전자흡인성의 3-크로몬알데히드류와 전자공여성의 2,2-이치환하이드라존류의 공액구조를 가지고 있다. 합성한 물질은 각각 FT-IR, $^1H-NMR$ 스펙트럼으로부터 그의 구조적 특성을 확인하였고, 융점, 수득률에 의하여 열적 안정성, 반응성을 확인하였으며, 여기스펙트럼과 발광스펙트럼으로부터 자외가시광과 발광특성을 확인하였다.

Purification and NMR Studies of RNA Polymerase II C-Terminal Domain Phosphatase 1 Containing Ubiquitin Like Domain

  • Ko, Sung-Geon;Lee, Young-Min;Yoon, Jong-Bok;Lee, Weon-Tae
    • Bulletin of the Korean Chemical Society
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    • 제30권5호
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    • pp.1039-1042
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    • 2009
  • RNA polymerase II C-terminal domain phosphatase 1 containing ubiquitin like domain (UBLCP1) has been identified as a regulatory molecule of RNA polymerase II. UBLCP1 consists of ubiquitin like domain (UBL) and phosphatase domain homologous with UDP and CTD phosphatase. UBLCP1 was cloned into the E.coli expression vectors, pET32a and pGEX 4T-1 with TEV protease cleavage site and purified using both affinity and gel-filtration chromatography. Domains of UBLCP1 protein were successfully purified as 7 mg/500 mL (UBLCP1, 36.78 KDa), 32 mg/500 mL (UBL, 9 KDa) and 8 mg/500 mL (phosphatase domain, 25 KDa) yielded in LB medium, respectively. Isotope-labeled samples including triple-labeled ($^2H/^{15}N/^{13}C$) UBLCP1 were also prepared for hetero-nuclear NMR experiments. $^{15}N-^{1}H$ 2D-HSQC spectra of UBLCP1 suggest that both UBL and phosphatase domain are properly folded and structurally independent each other. These data will promise us further structural investigation of UBLCP1 by NMR spectroscopy and/or X-ray crystallography.